PREPARATION OF HALOGENO ALKANE1)Suitable quantities of red phosphorus and butan-1-ol are placed in a roundbottomed flask fitted with a reflux

condenser.
Iodoalkanes cannot be made from sodium iodide and sulfuric acid; red phosphorus
and iodine can be used instead as the halogenating agent. if concentrated sulfuric
acid was added to solid sodium iodide? Give two observations-Misty /steamy
fumes, purple fumes, yellow solid deposite, black/purple solution.
sodium iodide and sulfuric acid cannot be used to make iodoalkanes from alcohols.
Because, There is little / no HI formed (which is the reagent needed) and HI is
oxidized to iodine.

2. The mixture is heated until it boils gently and then the heat source is removed.
3. A suitable quantity of powdered iodine is added in small portions down the
condenser at a rate which just maintains gentle boiling. The reaction should be
allowed to subside after each addition.
the way iodine is added, this nature of reaction is called exothermic.
4. After the addition of iodine is complete, the mixture is heated under reflux for
30 60 minutes, until little or no iodine is visible.
check there is no iodine visible by disappearance of purple coulour.
5. The apparatus is allowed to cool and the condenser rearranged for distillation.
6. The crude 1-iodobutane is distilled off until the residue in the distilling flask is
about one-fifth of its original volume. Double its volume of water is added and the
distillation continued until no more oily drops condense into the receiver.
7. The crude 1-iodobutane is separated and washed with dilute sodium thiosulfate
solution and then with dilute sodium carbonate solution.
it is washed with sodium thiosulfate to remove excess iodine.
8. The organic layer is separated and allowed to stand over anhydrous calcium
chloride.

calcium chloride must be anyhydrous because iti s a drying agent and it removes
excess water.
9. Distillation / re-distillation (over a narrow range of temperature) (either side of
the
boiling temperature of 1-iodobutane) to ensure the purity of 1-iodobutane.

enthalpy changeUsing the same equipment, together with a stop clock, suggest a
procedure that would improve the accuracy of this experiment by
obtaining a more accurate temperature change.-the mass of zinc and
volume of copperii sulfate is same.
Measure the temperature (of copper(II) sulfate) every minute / at realistic time
interval (15 s to 1
minute) for e.g. 2 4 minutes before adding zinc.
Measure temperature each minute / at realistic time intervals (after adding zinc) for
several minutes.
Note These readings may be started after the maximum temperature is reached /
after reaction has stopped and taken until the mixture has cooled to room
temperature. Intervals should be chosen to allow at least 4 readings on cooling
section of curve.
Plot a temperature - time graph / plot a graph using measurements (of temp and
time) obtained
Extrapolate to find T / maximum temperature (at the time of mixing ) Use
properly described intersecting lines to find maximum temperature

If zinc is added in small portions or over a period of time only first and third marks
can be awarded (Since measurements of cooling will be incorrect and there is no
definite time when reaction starts)
Use (finely) powdered magnesium hydroxide Use moderately concentrated acid /
acid which is not very dilute/ acid of higher concentration / keep excess acid to
minimum possible volume. Ensure good mixing / stir mixture
Any two improvements from use a lid on the crucible heat to constant mass
heat with a gentle/blue flame use a larger mass of crystals cool in a dry
atmosphere repeat experiment electrical heating

Why is it important that the temperature readings are taken as quickly as possible?
Temperature is taken before heat loss occurs / before mixture cools

Thermometric titrations can also be carried out using an electronic probe connected
to a computer, instead of a thermometer. The sodium hydroxide is run into the acid
from the burette at a steady rate. The acid is in an insulated beaker with a
magnetic stirrer. The computer then produces a plot of the results. Explain why this
modified method can give improved results, other than because of any increase in
accuracy of the temperature readings by the electronic probe.

Temperatures are monitored continuously

Equivalent to having more / many readings More points give a more accurate line /
plot
Magnetic stirrer more efficient than manual stirring / stirring is more uniform /
Heat loss is reduced because reaction is completed more quickly / because there is
no time delay in readings

Explain why more concentrated solutions are used in thermometric titrations.

To make temperature (change) bigger
To make more exothermic so more heat is given out
To reduce percentage error in temperature (change)
Give oneassumption made when calculation enthalpy changesno heat loss
reaction is complete
capacity of the solution is same as water
density of solution is 1.00gcm3.

less concentrated sodium hydroxide is irritant. More concentrated is corrosive, burns

the skin.

preparations of ketoneButanone, CH3 COCH2 CH3 , can be prepared from butan-2-ol, CH3 CH(OH)CH2 CH3
, using the procedure below. An organic solvent suitable for this procedure has a low
boiling temperature and is extremely flammable, so adequate safety precautions
must be taken.
Procedure 1. Place about 10 g of sodium dichromate(VI) and 20 cm3 of distilled
water in a conical flask. Shake the flask to dissolve the solid. Then slowly add about
8 cm3 of concentrated sulfuric acid.
2. Dissolve 5.00 g of butan-2-ol in the organic solvent in a round-bottom flask. Stand
the flask in a large beaker containing ice and water. Slowly add the acidified sodium
dichromate(VI) solution through a funnel to the butan-2-ol solution in the flask.
What colour change will be seen when the acidified sodium dichromate(VI) reacts
with the butan-2-ol? From orange to green.

The reaction is exothermic. Other than the risk of explosion, why is it important to
cool the flask in a beaker of ice and water in step 2? To prevent solvent boiling and
escape from the mouth of the flask.
3. When the addition is finished, leave the mixture to cool and separate the organic
layer, which contains the butanone, from the aqueous layer.
4. Wash the organic layer with sodium hydrogencarbonate solution , and then with
water. Discard the aqueous layer.
State the purpose of washing the crude butanone with sodium hydrogencarbonate
solution- removes excess acid.
Describe the method used to carry out this process, naming the piece of apparatus
used.
Put in a (stoppered) separating funnel / tap funnel with sodium hydrogencarbonate
(and shake the mixture) and Open the tap at intervals

5. Add some sodium sulfate, Na2 SO4 , to the organic layer and wait until this
solution is clear.
What is the purpose of adding sodium sulfate- drying agent removes water.
6. Decant the solution into a flask, and add a few anti-bumping granules.
7(6).Use distillation to remove the solvent, which has a lower boiling temperature
than butanone. The solvent boils between 32C and 36C.
Draw a labelled diagram of the apparatus used in step 6 to distil off the solvent from
the organic layer. The diagram should show at least one precaution which must be
taken when distilling an extremely flammable liquid.
Suitable flask (round bottom or pear shaped) fitted with stillhead, and with
thermometer in correct position with bulb opposite opening to condenser
Condenser angled downwards with correctly drawn inner tube and (water cooled)
outer tube
Collecting flask with vent in flask or in connection to it
Electrical heater( precaution)

First mark Apparatus should not be completely sealed / put vent in apparatus /
leave gap between condenser and receiving flask / insert gas outlet / use receiving
flask with opening (1) ALLOW Open end of apparatus for pressure release Second
mark Move (bulb of) thermometer to opposite opening to condenser

(anhydrous) calcium chloride / CaCl2 / magnesium sulfate / MgSO4 / sodium

sulphate / Na2SO4-drying agent
Separating funnel with tap (and stopper) ALLOW Any shaped tube with opening at
top which can be stoppered and tap at bottom (1) Cyclohexene in upper layer (1)
Dont penalise if labelled cyclohexane, not ene.